MELTING

SPECTRO ANALYSIS

CHEMICAL ANALYSIS

SPECTROMETER
Ir G HENDERIECKX
GIETECH BV

CONTENT
1.
2.
3.
4.
5.

INTRODUCTION
EQUIPMENT
OPERATION
SAMPLES
CONCLUSION

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

1. INTRODUCTION
The international standards do require mostly a chemical composition for the cast
metals, except for iron. But even if not required, the foundry does have an instruction
(or specification) about the chemical composition, adapted to the wall thickness and
required mechanical properties.
In order to prove that the delivered metal does comply with the requirements,
internationally accepted test equipment and procedures are required.
The spark light emission spectrometer is one of them.
But as common for all test equipment, a proper use is necessary. This means
calibration, standardisation and sampling.
A correct instruction must be available and followed by the operators.
The standardisation and calibration must be properly done and suite with the metals
to investigate.
To do this properly, good standardising and calibration samples are required. These
can be purchased with certificate and or produced by the foundry itself.

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

2. EQUIPMENT
The spark light emission spectrometer has changed from large fragile equipment to a
much smaller and less demanding equipment.
Before, there was a necessity for constant
temperature and humidity in very small range, which
required special precautions and extra investment.
Nowadays the required range for temperature and
humidity are larger and a regular executed
standardisation can compensate the differences.

The main part of the spectrometer is a vacuum chamber, flushed with Ar (argon)
before use.

The light, emitted by the sparking of the sample,

is detected by its entrance concerning wave
length per element. The photomultiplier tubes
are positioned on a curved bar.

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

The number of elements that can be tested is depending on the number of tubes.
Some elements do need more tubes, especially when large ranges are to be tested.
Example: Ni in the range of 0 to 5 % and another from 5 to 40 % and chromium in the
low range (< 2 %) and the high range (> 18%).

The second part is the spark table, consisting of an electrode and a connection with
the vacuum main part. The table must be cleaned after each spark and the sealing
must be correct.
If there is too much air leakage, the result will
not be correct.
If the table area is not clean, this can involve
the result too.

The tubes are detecting the light, particular for their wave length and transform the
detected amount into electrical charge. This amount of electricity is related to the
amount of the element in the metal.
With standard and calibration samples, the relation from the amount of electrical
charge to the element concentration in the sample, is set.
The third part is the computer, which will calculate, show, print and file result
according to the wish of the foundry. Some of them can directly print certificates.

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

3. OPERATION
The operation is only possible if first the equipment is properly standardised and
calibrated.
3.1 Standardising and calibrating
When the equipment is installed, the standardising is necessary.
This involves that for each type of metal, the response curve from each tube
(element) is related to the real chemical composition.
Two items are important:
1.

metals must be classified in groups with similar chemical compositions:

unalloyed and low alloyed iron, unalloyed and low alloyed steel, high
alloyed iron (per type of alloy), high alloyed steel (per type of alloy)

2.

the standardising is only valid for the range between the lowest and
highest value, per element, from the used standards. A little
extrapolation can be done but with care!

It is impossible to perform proper tests for concentrations way outside of the

standards range. This is very important for S, P, Mg, Ce a nd it is mostly forgotten for
testing the residual elements like Pb, Ti, As, Sb, B
It is impossible to test elements in iron with a program that is standardised with steel
samples.

Each morning, or before each different material test, the equipment must be
calibrated.
This is necessary because due to the temperature and humidity, the equipment can
change (length between the tubes and zero point of the equipment is deciding about
the testing and this length can change).
It is important to calibrate with the proper test samples (equal metal or very similar
concerning analysis).
This calibrating can be done with other samples as for the standardising, but keep in
mind that the accuracy of the test will depend on the accuracy of the analysis of the
calibration sample.
It is necessary to set up a SPC (standard process control) system to detect
systematically appearing errors and shifting trends.

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

The accuracy of the test is depending on the accuracy of the standardising and
the calibrating. Both have an equal importance and should be done with the
highest care!

3.2 Testing
The testing itself will involve the following operations:
1. Sample Taking Procedures
Is this consistent, which means with the same quick chilling, resulting in a
white metallurgical structure?
Is the sample without slag or other inclusions?
Is the sample taken at the same time, which means that the metal:

must be homogenised
is taken equal depth under the metal surface
is taken at about the same time after switching power off, or after
tapping or after a metallurgical treatment.

2. Sample preparation
The method should be equal as used for standardising and calibrating. It can
be wet or dry grinding.
The surface must be flat.
The grinding must remove surface
scale, oxides and all oil and other
residues.
The operator must check the presence
of slag, porosity, inclusions

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

3. Operators technique
The operator must work according to the instructions, which include:
check if the equipment is properly calibrated
check that Ar properly supplied
check that flatness and quality of the
sample
check the preburn time
check the burn-spot in homogeneity
burn at least 2, preferred 3 times
never burn overlapping (one overlaps a
previous one).
The operator should check for abnormal results (very different from the other)
and try to find the cause. Eventually make a new burn and eliminate the
abnormal one.
Check the average result with the calculated (or expected) result.

4. Reporting
The melting and or pouring crew must be reported very quickly in order to
enable them to correct the chemical analysis before pouring.
File the results per melting charge with the history (number and amount of
corrections performed during the operation).
The results can also be filed and used to make reports and or certificates.
Take care to correct the result with the additions of elements due to
metallurgical treatments like inoculation, de-oxidising

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

4. SAMPLES
There are several types of samples:
1. High accuracy, certified sample
This sample must be used for the first and later standardisations. It
must be bought with a valid certificate of analysis and tolerance range.
It is very expensive and will be used restrictedly.
2. Calibration sample
This sample is certified with analysis and tolerance range. It is used for
the daily certification and is less costly.
3. Reference sample
This is a sample, mostly produced by the foundry, which is tested
according to the calibration samples. It is less accurate but sufficiently
for the day to day use.
In case of doubt, the calibration sample can be used.
The first very important remark is that iron can only be tested if it is white solidified! It
cannot be tested with a sample cut from the casting!
The samples must include the expected and tested concentration of every element in
the standardising and calibration range.
Pay attention for important residual elements, which are mostly present in a very low
concentration, which exceeds the range of the calibration and even sometimes the
standardisation samples.
Incorrect burns (overlapping, including moisture or oil, not white solidified sample)
must be removed immediately from the file.
4. Production sample
The spectrometer sample is 30 mm diameter and 6 mm thick. It is
poured in a copper book mold for fast chilling of the sample. The
sample must be fully chilled.
It must be clean and smooth, equal surface to avoid leakage.

Ir G.D HENDERIECKX

GIETECH BV

September 2006

MELTING
SPECTRO ANALYSIS

5. CONCLUSION
The result of the chemical analysis test with a spark light emission spectrometer is
depending on the proper use of the equipment, the correct standardisation and
calibration for the metal involved and the correct sample preparation.
In a lot of foundries, the testing is done without the necessary care of calibrating and
performing a proper test.

Ir G.D HENDERIECKX

GIETECH BV

September 2006